The method of producing vinyl chloride by catalytic pyrolysis of dichloroethane

 

(57) Abstract:

Use: an intermediate in industrial organic synthesis. The inventive dehydrochlorination of 1, 2-dichloroethane in the presence of a heterogeneous catalyst. Process conditions: temperature 350 - 490oWith the passing with the contact time is 0.1 to 5.0 with a mixture of EDC vapor with an inert gas (argon or nitrogen) in a volume ratio of N2: EDC = (0,0 - 2,0): 1,0 through a reactor filled with catalyst, the ratio of the volume of the catalyst: the volume of the reactor (0,15 - 1,0): 1,0. Periodically instead of filing EDC reactor rinsed with hydrogen and the ratio of the length of the feed EDC for the duration of the supply of hydrogen (0.5 to 10): 1,0. As catalyst, use of the porous carbon material in which layers of carbon are oriented in space in the form of a face of the polyhedron with the surface of the basal planes having the following structural characteristics: interlayer distance d002 - 0,34 - 0,349 nm, the size of microcrystallites in the direction "a", La = 3.0 to 12 nm, in the direction "c" Lc = 3.0 to 8 nm, specific surface of 12 - 650 m2/, this increases the productivity of the process and the output of REF. 5 C. p. F.-ly, 5 PL.

The invention atozlistings to clean emissions disposal of the toxic compounds and produce useful products, in particular the processing of 1,2-dichloroethane with the aim of obtaining vinyl chloride.

The process of transformation of EDC in I based on the reaction of removal of hydrogen chloride at elevated temperature:

CH2ClCH2Cl CH2= CHCl+HCl

A known number of patents in which they proposed to carry out the pyrolysis of dichloroethane (EDC) on solid catalysts. For example, in [1] the EDC pyrolysis is performed on the catalyst MgCl2/Al2O3when the ratio of Mg, Al (0.2 to 0.5):1 for 2 h at atmospheric pressure, a temperature of 400aboutWith and feed speed EDC 13 h-1that provides a contact time of 5.7 C. the Yield of vinyl chloride (I) is 56,3 wt.

In [2] as a catalyst used chloride of cobalt supported on alumina. The EDC pyrolysis is carried out at 350-400aboutC and a contact time of 5.7 C for 4 h, followed by regeneration of the catalyst with air purge for 2 hours depending on conditions, the degree of conversion of EDC in I ranges from 50 to 60 wt. (similar).

The main drawback of these methods is the low selectivity of the process, which does not allow to obtain high yield of the target product of the performance process. Periodic removal of these products by calcining the catalyst in air flow though and restores the efficiency of the process, but creates a new problem of disposal of highly toxic chlorinated compounds formed during the incomplete combustion products resinification catalyst.

Patent [3] and the scientific literature [4, 5] it is used as a catalyst pyrolysis of EDC active carbons having turbostrategy structure (with chaotic output end surface and basal faces of microcrystallites carbon, and x-ray amorphous carbon formations) with a specific surface area 727 1100 m2/g pre-processed in the current CO2, air or a mixture of CO2with air at 950aboutC. the closest to the technical nature of the claimed method is dehydrochlorinating EDC [4] (prototype), which consists in passing the vapors through EDC reactor filled with activated carbon with a specific surface area of between 100 to 700 m2/year contact Time EDC is 26 C. the process Temperature of 300-400aboutC. Under these conditions, the degree of conversion of EDC is to 94.5 mol. Significant disadvantages of this method are the low productivity of the process, and Thai education I.

The objective of the proposed method of producing vinyl chloride is greater productivity and increased output I.

This object is achieved in that the process is carried out at 350-490aboutTransmission by contact time is 0.1 to 5.0 with a mixture of EDC vapor with an inert gas (argon or nitrogen) in the volume ratio of N2DHA,0-2,0:1,0 through a reactor filled with a catalyst in the ratio of the volume of catalyst/volume of reactor (0,15-1,0): 1,0. As catalyst, use of the porous carbon material in which layers of carbon are oriented in space in the form of a face of the polyhedron with the surface of the basal planes and having the following structural characteristics: interlayer distance d002= 0,34-0,349 nm, the size of microcrystallites in the direction of "and" La 3,0-12 nm in the direction "C" Lc 3,0-8 nm, specific surface 12-650 m2/,

Distinctive features in comparison with the known methods of obtaining the I are the use as catalyst of a new carbon-graphite material, the surface of which is formed from the basal planes of microcrystallites carbon and having an interlayer distance d002 0,34-0,349 nm, the size of microcrystallites directed by the RTO is the process on the specified catalyst is carried out at 350-490aboutC. the Next difference is that the contact time is 0.1 to 5.0 C. Another difference is that EDC is introduced into the reactor in the form of a mixture with an inert gas (argon or nitrogen) in the volume ratio of N2EDC 0,0-2,0 1,0. The next difference is that the reaction volume of the reactor is filled with catalyst in proportion to the volume of catalyst/volume of reactor 0,15-1,0: 1,0. The next difference is that periodically instead of filing EDC reactor rinsed with hydrogen and the ratio of the length of the feed EDC for the duration of the supply of hydrogen is 0.5-10:1,0.

The choice of these parameters of the process due to the peculiarities of the reaction pyrolysis of EDC, including the stage of interaction of the reagent with the surface of the solid catalyst and the flow of radical processes in the reactor volume.

Below are examples of the implementation process of the prototype and the proposed method.

P R I m e R 1 (prototype). Experiments on the pyrolysis of EDC is carried out in a flow quartz reactor with a volume of 7 cm3with internal thermocouple pocket at atmospheric pressure. The reactor was loaded a portion (3.0 g) active in the m Lc 2,3 nm, d002 0,356 nm. In the reactor serves pairs EDC with a bulk velocity, providing a contact time of 1 C. the reaction Temperature 400aboutC. the Degree of conversion of EDC to determine out by a titrimetric method for the number formed in the pyrolysis of HCl. The composition of the gas phase to determine the chromatographic method. The duration of the experiment 50 minutes

The degree of conversion of EDC is 5.0%, the Selectivity of the formation of I is 85%

After completion of the pyrolysis of EDC (50 min) carry out the activation of the catalyst by the method of [5] To do this, stop filing EDC, the reactor purge air for 15 min and then served EDC. After activation of the catalyst, the degree of transformation EDC is 5.0%, the Selectivity of the formation of I is 86%

P R I m m e R 2. Similar to example 1 with the difference that the catalyst used porous carbon material in which layers of carbon are oriented in space in the form of a face of the polyhedron with the surface of the basal planes and having the following structural characteristics: interlayer distance d002 0,349 nm, the size of microcrystallites in the direction of "and" La 3,0 nm in the direction "C" line with an of 3.0 nm, a specific surface area of 650 m2/year and stop in the reactor for 50 min serves EDC with a contact time of 1 sec.

The degree of conversion of EDC is 55%, the Selectivity of the formation of I is 98%

P R I m e R 3. Similar to example 1 with the difference that the catalyst used porous carbon material in which layers of carbon are oriented in space in the form of a face of the polyhedron with the surface of the basal planes having the following structural characteristics: interlayer distance d002 0,345 nm, the size of microcrystallites in the direction of "and" La 4,2 nm in the direction "C" Lc= 3,5 nm, specific surface area of 33 m2/, Through the reactor at 405aboutC for 15 min miss hydrogen with a contact time of 1 sec. Then the supply of hydrogen is stopped and the reactor for 50 min serves EDC with a contact time of 1 sec.

The degree of conversion of EDC is 55%, the Selectivity of the formation of I is 98%

P R I m e R 4. Similar to example 1 with the difference that the catalyst used porous carbon material in which layers of carbon are oriented in space in the form of a face of the polyhedron with the surface of the basal planes and having the following structural characteristics: interlayer distance d002 0,340 nm, the size of microcrystallites in the direction of the 15 min miss hydrogen with a contact time of 1 C. Then the supply of hydrogen is stopped and the reactor for 50 min serves EDC with a contact time of 1 sec.

The degree of conversion of EDC is 15%, the Selectivity of the formation of I is 98%

P R I m e R 5. Similar to example 1 with the difference that the catalyst used porous carbon material in which layers of carbon are oriented in space in the form of a face of the polyhedron with the surface of the basal planes and having the following structural characteristics: interlayer distance d002 0,345 nm, the size of microcrystallites in the direction of "and" La 4,2 nm in the direction "C" Lc= 3,5 nm, specific surface area of 33 m3/, Through the reactor at 490aboutC for 15 min miss hydrogen with a contact time of 1 sec. Then the supply of hydrogen is stopped and the reactor for 50 min serves EDC with a contact time of 1 sec.

The degree of conversion of EDC is 98% selectivity of the formation of I is 90%

Examples 6-10 illustrate the process with periodic replacement of the supplied EDC for argon, oxygen and hydrogen.

P R I m e R 6. Similar to example 1 with the difference that the catalyst used porous carbon material in which layers of carbon eusi the following structural characteristics: the interplanar rasstoyane d002 0,345 nm, size microcrystallites in the direction of "and" La= 4,2 nm in the direction "C" Lc 3,5 nm, specific surface area of 33 m2/, Through the reactor at 400aboutC for 15 min miss hydrogen with a contact time of 1 sec. Then the supply of hydrogen is stopped and the reactor for 50 min serves EDC with a contact time of 1 C. the Degree of conversion of EDC is 53%, the Selectivity of the formation of I is 98% then stop filing EDC, the reactor serves argon with a contact time of 1 s for 10 min and then served EDC for 50 min. Through 80 hours of work in this mode, the degree of conversion of EDC is 29%, the Selectivity of the formation of I is 98%

P R I m e R 7. Similar to example 1 with the difference that the catalyst used porous carbon material in which layers of carbon are oriented in space in the form of a face of the polyhedron with the surface of the basal planes and having the following structural characteristics: interlayer distance d002 0,345 nm, the size microcrystallites direction "and" La=4,2 nm in the direction "C" Lc 3,5 nm, specific surface area of 33 m2/, Through the reactor at 400aboutC for 15 min miss hydrogen with a contact time of 1 sec. Then the flow of hydrogen ceased the awn education I is 98% then stop filing EDC, into the reactor an oxygen with a contact time of 1 C for 5 min and then served EDC within 50 minutes the Degree of conversion of EDC is 3.9%

P R I m e R 8. Similar to example 1 with the difference that the catalyst used porous carbon material in which layers of carbon are oriented in space in the form of a face of the polyhedron with the surface of the basal planes and having the following structural characteristics: interlayer distance d002 0,345 nm, the size of microcrystallites in the direction of "and" La 4,2 nm in the direction "C" Lc 3,5 nm, specific surface area of 33 m2/, Through the reactor at 400aboutC for 15 min miss hydrogen with a contact time of 1 sec. Then the supply of hydrogen is stopped and the reactor for 50 min serves EDC with a contact time of 1 C. the Degree of conversion of EDC is 53%, the Selectivity of the formation of I is 98% then stop filing EDC, the reactor serves hydrogen with a contact time of 1 C for 100 min and then served EDC. After 80 hours of operation in this mode, the degree of conversion of EDC is 55%, the Selectivity of the formation of I is 98%

P R I m e R 9. Same as example 8 with the difference that the temperature of the treatment with hydrogen composition is adowanie I is 98%

P R I m e R 10. Same as example 8 with the difference that the temperature of the treatment with hydrogen is 600aboutAnd the processing time of 5 minutes the Degree of conversion of EDC is 52%, the Selectivity of the formation of I is 98%

Examples 11 to 15 illustrate the effect of the modes of supply EDC.

P R I m e R 11. Similar to example 3 with the difference that the temperature of the treatment with hydrogen 550aboutWith the duration of 15 min and the EDC pyrolysis is carried out at 400aboutC for 4 h, the Degree of transformation EDC is 48%, the Selectivity of the formation of I is 97%

P R I m e R 12. Similar to example 3 with the difference that the temperature of the treatment with hydrogen 550aboutWith the duration of 15 min and the EDC pyrolysis is carried out at 400aboutC for 2 h, the Degree of transformation EDC is 51%, the Selectivity of the formation of I is 98%

P R I m e p 13. Similar to example 3 with the difference that the temperature of the treatment with hydrogen 550aboutWith the duration of 15 min and the EDC pyrolysis is carried out at 400aboutC for 50 min with a contact time of 0.1 C. the Degree of conversion of EDC is 16%, the Selectivity of the formation of I is 98%

P R I m e R 14. Similar to example 3 with the difference that the temperature of the treatment with hydrogen 550The degree of conversion of EDC is 35%, the Selectivity of the formation of I is 98%

P R I m e R 15. Similar to example 3 with the difference that the temperature of the treatment with hydrogen 550aboutWith the duration of 15 min and the EDC pyrolysis is carried out at 400aboutC for 50 min with a contact time of 5.0 C. the Degree of conversion of EDC is 63%, the Selectivity of the formation of I is 97%

P R I m e R 16 (optimum process). Same as example 8 with the difference that the temperature of the treatment with hydrogen is 520aboutAnd the processing time of 15 minutes, the pyrolysis Temperature of 450aboutC. the duration of the pyrolysis of 2 hours Through 10 hours of work, the degree of transformation EDC is 81%, the Selectivity of the formation of I is 97%

Examples 17-19 illustrate the influence of the degree of filling of the reactor with the catalyst.

P R I m e R 17. Similar to example 16 with the difference that the ratio of the volume of catalyst/volume of reactor is 0.75. The degree of conversion of EDC is 83%, the Selectivity of the formation of I is 97%

P R I m e R 18. Similar to example 16 with the difference that the ratio of the volume of catalyst/volume of the reactor is 0.5. The degree of conversion of EDC is 80% selectivity of the formation of I is 97%

P R I m e R 19. Similar to example 16 with the difference that soothes the education I is 98%

Examples 20-22 illustrate the effect of dilution EDC inert gas.

P R I m e R 20. Similar to example 16 with the difference that in the reactor serves a mixture of argon and EDC in the ratio 1:2. The degree of conversion of EDC is 85% selectivity of the formation of I is 97%

P R I m e R 21. Similar to example 16 with the difference that in the reactor serves a mixture of argon and EDC in 1:1 ratio. The degree of conversion of EDC is 90% selectivity of the formation of I is 96%

P R I m e R 22. Similar to example 16 with the difference that in the reactor serves a mixture of argon and EDC in a 2:1 ratio. The degree of conversion of EDC is 86% selectivity of the formation of I is 97%

Thus, the proposed method allows to increase the productivity of the process of pyrolysis of EDC and output REF. Also essential is the possibility of long-term maintenance of high productivity due to the periodic purging of the reactor with hydrogen.

Characteristics of the method of producing vinyl chloride by catalytic pyrolysis of dichloroethane in examples 1-22 are presented in table.1-5.

1. The METHOD of producing vinyl CHLORIDE by CATALYTIC PYROLYSIS of DICHLOROETHANE by passing vapors through a reactor filled katal is terasawa material using porous graphitized carbon material, in which layers of carbon are oriented in space in the form of a face of the polyhedron with the surface of the basal planes with interplanar distance d 002 equal 0,34 - 0,349 nm, the size of microcrystallites in the direction of a Laequal to 3.0 to 12 nm, in the direction of c lcequal to 3,0 to 8 nm, a specific surface area of 12 - 650 m2/,

2. The method according to p. 1, wherein the process is carried out at 350 - 490oC.

3. The method according to p. 1, characterized in that the dichloroethane is passed through the reactor at a contact time of 0.1 to 5.0 C.

4. The method according to p. 1, characterized in that the dichloroethane is passed through the reactor in a mixture with an inert gas in the volume ratio of inert gas-dichloroethane, equal to 0,9 - 2,0 : 1,0.

5. The method according to p. 1, otlichayushiesya the fact that the process is conducted in a reactor filled with a catalyst, the ratio of the volume of the catalyst: the volume of the reactor, 0.15:1,0:1,0.

6. The method according to p. 1, wherein the process is conducted at periodic purging the reactor with hydrogen instead of filing dichloroethane at a ratio of the length of the transmission dichloroethane and hydrogen of 0.5 - 10 : 1,0.

 

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